Process for the rapid fixing of ethylene by means of sulphuric acid for the purpose of obtaining neutral ethyl sulphate



so the present patent a ing at ,least 97% of 4 0 added as catalyzeracompound of a comlency, for 50 FeSO, (and not am; Sept. 7, 1926.

UNITED STATE 5 PATENT orrlcs.

nuqus'rm AIEDIEE Louis .rosnrn nainnns, or swans-trams CHARLES jlrosnrnELYSEE m: LOISY, or rams, rmmcn, Arm OLIVIER :rosnrn GISLAIN rrn'r'rn,on

BRUSSELS, BELGIUM.

rnocnss ron'run M211) rrxme or: ETHYLENE BY MEANS or SULPHUBIC ACID sonrim runrosn or on'ramme NEUTRAL ET-HYL SULI'HATE.

'80, Drawing. Original application fi led April is, 1922, semi No.552,306, and in at June 2, 1921.

I Divided and this application filed September 5, 1923. Serial No.661,090.

Thepresent application is adivision of our patent, application SerialNo. 552,306,

filed April 13th, 1922 relating to a process for the rapid fixing ofethylene by means of 5 sulphuric acid fO1 th6pllIpOSB of obtaining"which application has 1 ethyl sulphuric esters, resulted in the grant ofLetters Patent No. 1,574,796 dated March 2, 1926. p a I The presentapplication relates to a process' for the rap1d fixing of ethylene bymeans ofsulphuric acid for the purpose of obtaining neutral ethylsulphate.

'Various authors among Sidgwick, as well as Henry R. Curme, have 15shown that it is possible to obtain neutral eth l sulphate by the actionof sulphuric aci on ethglene under the influence of heat; Plant andidgwick have shown that by operating'at a temperature from 50 to 70-:00. neutral ethyl phate relatively to the ethylene used is thereforevery small since a large portion of the ethglene is used up to. formethyl sulphuric aci r The process forming, the subject-matter ofpflication allows, on

the contrary, to manu acture'neutral ethyl sulphate starting fromethylene or from the complex gas which contains the latter, on acommercial scale and with an output as high aspossible;

' This process consists essentially in treat-- ing ethylene, or thecomplex gas which contains the latter, with sul huric acid contain- S0to which is mon metal containing the"meta'l-.u'nder its smallestvalency, reactgm being maintained between 0 and y 1 v v The process ischaracterized essentially by the use of a catalyzer composed of iron,

uivalent common or base metal a metal under its smallest va instance aferrous compound a ferric compound such as Fe,(SO,),), a cuprouscompound (and not PP 1 containing t a cupric compound them Plant and.

the temperature during the such as Sub-chloride of copper Cu l su oxideof copper Cu O, sub-sulphate of copper Cu S O etc., or any compoundscapableof givin them birth, for instance, copper sulphate uSO, and areducing body which will transform it into on rous sulphate Cu SO uringthe reaction of ethylene in presence of the above mentioned catalyzer,the temperature must be maiiltained between 0 and 15 C. as above setforth; the output in neutral ethyl sulphate will be the higher, thenearer the temperature approachesO The operation of fixing ethylene iscontinued until the reagent is saturated with the gas and ceases toabsorb' it.

sulphuric n acid on At the end of the 0peration,the acid is diluted andthe neutral ethyl sulphate is collected, this neutral ethyl sulphatefloatmg on thesurface of the sulphuric acid which retains in solution avery small pro portion only of ethylsulphuric acid.

advantages:

1The absorption of ethylene is efi'ected with great rapidity and owingto the low temperature at which the process is carried out, thesulphuric acid does not substantially exert any prejudicial action onthe-products formed. e

-The catalyzin body is ,a com-- mon and cheap product.

3--This catalyzing body is insoluble in sulphuric acid, whichdifierentiates it from the old process.-

the catalyzers used up to this day which were soluble. The considerableadvantages eonnected with this property are, on the one hand, that thegreater division of the acid is promoted by the presence in its mass ofa recipitate in suspension and, on the othe;

and, thatthe catalyz'er can easily be colwas lected at the end of theoperation, by decantation, filtration or centrifuging, and be used overagain for subsequent reactions For carrying out the present process inthe case of its application to the trapping of ethylene contained inindustrial gases: natural gas, gas from the distillation of fuels (cokeoven gas, illuminating gas, cracking gas, schist gas, syntheticethylene, etc.) it is preferable first to free these gases from benzoland ammonia, to dehydrate them and, generally speaking, ,to free themfrom products which might be objectionable on account of their actioneither on the acid or on the catalyzing body (hydrocarbons of theacetylene and ethylene series, homologues of ethylene, sulphuratedcompounds, etc.).

The reagent fixing the ethylene (sulphuric acid to which is added thecatalyzing body) is after absorption, subjected to a decantation,filtration or centrifuging, so that the catalyzing body can be collectedand can be introduced into the circulation afterlor withoutpurification.

While in the appended claims We have mentioned the use of coppercompounds as catalyzers, we desire it to be'understood acid containingat least 97% of H 0 a 'Augu compound containing copper in the monovalentstate,in causing a gaseous current containing ethylene to pass throughthis add,

the temperature being maintained between 40 0 and 15 C. during thereaction,separating the catalyzer from the acid, diluting the latter,and collecting the neutral ethyl sulphate which floats to the surface ofthe sulphuric acid, which latter retains in solution a very" smallproportion only of ethyl sulphuri c acid.

rent containing ethyleneto pass through this acid, the temperaturebeing'maintained between 0 and 15 C. during the reaction,- scparatingthecatalyzer from the acid, diluting the latter, and collecting theneutral ethyl sulphate which floats to the surface of the sulphuricacid, which latter retains in solution a very small proportion only ofethyl sulphuric acid.

The foregoing specification of our process for the rapid fixing ofethylene bymeans of sulphuric acid for the purpose of obtaining neutralethyl sulphate, signed at Paris, F rance, this 20th day of July 1923,by-

AUGUSTIN AMEDEE LOUIS JOSEPH 'DAMIENS. MARIE CHARLESJOSEPH ELYSEE deLOlSY. I and at Brussels, Belgium, this 14th day of' st 1923, by--OLIVIER JOSEPH GlSLAlN PlET'lE.

